In this study, expired egg white was used as a template, and a sol–gel method was employed to prepare pure-phase TiO2 nano-powder and mixed-phase powders doped with NaF and NaI. The influences of different calcination temperatures, doping elements, and doping amounts during the preparation process on the photocatalytic performance and activity of the prepared TiO2 powders were studied. The results of the experiments showed that the F-doped TiO2 had the highest photocatalytic activity when the doping amount was 1.2%, as examined by EDS, where the sintering temperature was 500 °C. F-doped TiO2 nanoparticles were also synthesized by the sol–gel method using tetrabutyl titanate and NaF mixed with expired egg white protein as the precursor. The F-TiO2 photocatalyst was characterized using FE-SEM, HR-TEM, EDS, XPS, and UV-Vis, and the photocatalytic activity was evaluated by photodegradation of methylene blue under visible light. The results showed that doping with F reduced the energy band gap (3.04 eV) of TiO2, thereby increasing the photocatalytic activity in the visible-light region. The visible-light wavelength range and photocatalytic activity of the catalyst were also affected by the doping amount.
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